The laboratory established an efficient reversed-phase ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)qualitative method for screening more than 2000 kinds of ris...The laboratory established an efficient reversed-phase ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)qualitative method for screening more than 2000 kinds of risk substances(including local anesthetics,LAs)in cosmetics,which has been successfully applied in the analysis of actual samples.This work aims to develop a more convenient high performance liquid chromatography triple quadrupole mass spectrometry(HPLC-QQQ-MS/MS)method for the quantitative determination of LAs.Samples were ultrasonically extracted with methanol,separated on an Agilent Poroshell 120 EC-C18 column(2.1 mm×100 mm,2.7μm),and eluted with a gradient mobile phase consisting of 0.1%formic acid aqueous solution and methanol.Quantification was performed using the external standard method.The results show that all 23 LAs are effectively separated within 12 minutes,with good linearity in the corresponding concentration ranges and the correlation coefficients all greater than 0.99.The limits of detection(LOD)range from 0.0025 to 0.05μg/g,and the limits of quantification(LOQ)range from 0.01 to 0.1μg/g.The average recoveries of the 23 LAs in 5 blank cosmetic matrices are 80.68%-117.57%,with the relative standard deviations(RSDs)less than 5.98%.This method has good precision and high accuracy,and is suitable for the determination of LAs in 5 cosmetic matrices.展开更多
目的 分析金雀花乙醇提取物的化学成分。方法 采用超高效液相色谱-四极杆-飞行时间串联质谱(Ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry, UPLC-Q-TOF-MS/MS)技术,使用A...目的 分析金雀花乙醇提取物的化学成分。方法 采用超高效液相色谱-四极杆-飞行时间串联质谱(Ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry, UPLC-Q-TOF-MS/MS)技术,使用ACQUITY UPLC BEH C18色谱柱,流动相为0.1%甲酸水溶液和乙腈,线性梯度洗脱;采用电喷雾离子源在m/z50~1 500范围内采集数据;采用UNIFI V 1.9.2软件对数据进行预处理、峰检测、分子式推测,通过高分辨质谱数据结合数据库、文献和对照品进行对比,分析金雀花乙醇提取物中的化学成分。结果 共分析出47种化学成分,包括27种黄酮类、13种皂苷类、7种其他类成分,其中包括山奈酚-3-O-芸香糖苷、牡荆素、金丝桃苷、山奈苷、水仙苷、芹菜素、槲皮素、金合欢素等成分。结论 本研究分析了金雀花乙醇提取物中的化学成分,为后续金雀花的开发与利用提供了理论基础。展开更多
文摘The laboratory established an efficient reversed-phase ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)qualitative method for screening more than 2000 kinds of risk substances(including local anesthetics,LAs)in cosmetics,which has been successfully applied in the analysis of actual samples.This work aims to develop a more convenient high performance liquid chromatography triple quadrupole mass spectrometry(HPLC-QQQ-MS/MS)method for the quantitative determination of LAs.Samples were ultrasonically extracted with methanol,separated on an Agilent Poroshell 120 EC-C18 column(2.1 mm×100 mm,2.7μm),and eluted with a gradient mobile phase consisting of 0.1%formic acid aqueous solution and methanol.Quantification was performed using the external standard method.The results show that all 23 LAs are effectively separated within 12 minutes,with good linearity in the corresponding concentration ranges and the correlation coefficients all greater than 0.99.The limits of detection(LOD)range from 0.0025 to 0.05μg/g,and the limits of quantification(LOQ)range from 0.01 to 0.1μg/g.The average recoveries of the 23 LAs in 5 blank cosmetic matrices are 80.68%-117.57%,with the relative standard deviations(RSDs)less than 5.98%.This method has good precision and high accuracy,and is suitable for the determination of LAs in 5 cosmetic matrices.
